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研究生:林廖梅英
研究生(外文):Mei-Ing Laiw
論文名稱:海藻中無機砷分析方法之探討
論文名稱(外文):Studies on Method for Determining Inorganic Arsenic in Marine Algae
指導教授:黃登福黃登福引用關係
學位類別:碩士
校院名稱:國立海洋大學
系所名稱:食品科學系碩士在職專班
學門:農業科學學門
學類:食品科學類
論文種類:學術論文
論文出版年:2002
畢業學年度:90
語文別:中文
論文頁數:64
中文關鍵詞:海藻類鹽酸蒸餾法無機砷石墨爐式原子吸收光譜儀
外文關鍵詞:Marine algaeHCl distillationInorganic arsenicGFAAS
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本研究利用鹽酸蒸餾法萃取,以側向加熱石墨管(Transverse heated graphite tube, THGT)之石墨爐式原子吸收光譜儀(Graphite furnace atomic absorption spectrophotometer, GFAAS)檢測,建立海藻中無機砷之檢驗方法。將海藻檢體加4 N鹽酸溶液及30%碘化鉀溶液,加熱蒸餾,餾出液以鎳硝酸溶液為基質修飾劑,以石墨爐式原子吸收光譜儀分析檢測,最適灰化溫度為1,100℃,最適原子化溫度為2,300℃。綠藻中添加砷10、20及30 ppm之平均回收率為92.9~93.2﹪,變異係數介於0.6~2.1%。分析20件食用海藻,9件褐藻無機砷平均含量為18.1 ppm (2.8~59.1 ppm),總砷平均含量為52.0 ppm (8.8~111.4 ppm) ;9件紅藻無機砷平均含量3.9 ppm (0.2~7.3 ppm),總砷平均含量為23.4 ppm (1.8~39.8 ppm),2件綠藻無機砷平均含量為0.5 ppm (<0.1~0.9 ppm),總砷平均含量為5.4 ppm (4.2~6.7 ppm)。

A method for assay of inorganic arsenic in marine algae was established. Inorganic arsenic was thermally distilled with HCl and then analyzed by Graphite Furnace Atomic Absorption Spectrophotometer (GFAAS) equipped with Transverse Heated Graphite Tube (THGT). The thermal distillation was done by addition of 4 N HCl 25 mL and 30% KI 10 mL, and the distillate was modified with Ni(NO3)2 matrix modifier. The optimum ashing temperature was 1,100C and the optimum atomization temperature was 2,300C. The recovery and variation coefficient for 10、20 and 30 ppm of arsenic spiked into Chlorophyta were 92.9~93.2% and 0.6~2.1%, respectively. The commercial algae included Phaeophyta (9 samples), Rhodophyta (9) and Chlorophyta (2) were collected from markets in Taiwan. The average levels of inorganic arsenic and total arsenic were 18.1 ppm (2.8~59.1 ppm) and 52.0 ppm (8.8~111.4 ppm) for Phaeophyta, 3.9 ppm (0.2~7.3 ppm) and 23.4(1.8~39.8 ppm) for Rhodophyta, and 0.5 ppm (<0.1~ 0.9 ppm ) and 5.4 ppm (4.2~6.7 ppm) for Chlorophyta, respectively.

頁次
中文摘要…………………………………………………………… 1
英文摘要…………………………………………………………… 2
壹、前言…………………………………………………………… 3
貳、文獻整理……………………………………………………… 7
一、砷的形態與毒性……………………………………………… 7
二、砷之攝入及代謝……………………………………………… 9
三、海藻中砷之含量……………………………………………… 11
四、無機砷之限量標準…………………………………………… 12
五、無機砷之分析方法…………………………………………… 14
(一)比色法………………………………………………………… 14
(二)氫化物產生系統原子吸收光譜儀…………………………… 15
(三)高效液相層析/氫化物產生系統原子吸收光譜儀………… 15
(四)高效液相層析/感應耦合電漿質譜儀……………………… 16
(五)毛細管電泳法………………………………………………… 16
(六)氣相層析法/質譜儀………………………………………… 17
(七)石墨爐式原子吸收光譜……………………………………… 17
1.石墨原子吸收光譜儀裝置與原理……………………………… 17
(1)系統裝置……………………………………………………… 17
(2)灰化及原子化升溫程序……………………………………… 18
(3)基質修飾劑使……………………………………………………18
2.利用石墨原子吸收光譜儀分析無機砷………………………… 19
六、文獻整理之圖表……………………………………………… 20
參、材料與方法…………………………………………………… 31
一、試藥與試劑…………………………………………………… 31
二、檢體來源……………………………………………………… 32
三、儀器設備與裝置……………………………………………… 32
四、標準溶液之調製……………………………………………… 33
五、試驗方法……………………………………………………… 33
(一)蒸餾條件之探討……………………………………………… 33
(二)GFAAS最適檢測條件之探討………………………………… 34
1.基質修飾劑之影響……………………………………………… 34
2.最適灰化及原子化溫度條件…………………………………… 34
3.不同價態砷標準曲線斜率之比較……………………………… 35
六、添加回收試驗………………………………………………… 35
(一)鹽酸溶液濃度之影響………………………………………… 35
(二)添加回收……………………………………………………… 36
七、偵測極限……………………………………………………… 36
(一)儀器偵測極限………………………………………………… 36
(二)方法偵測極限………………………………………………… 36
八、校正曲線法與標準添加法斜率之比較……………………… 36
九、參考樣品之驗證……………………………………………… 37
十、市售海藻類食品含量之分析………………………………… 37
(一)水分含量之分析……………………………………………… 37
(二)砷含量之分…………………………………………………… 37
肆、結果與討論…………………………………………………… 39
一、蒸餾條件探討………………………………………………… 39
二、GFAAS最適檢測條件之探討……………………………………39
(一)基質修飾劑之影響…………………………………………… 39
(二)不同價態砷標準曲線斜率之比較…………………………… 40
三、添加回收試驗………………………………………………… 41
(一)鹽酸溶液濃度之影響………………………………………… 41
(二)添加回收……………………………………………………… 41
四、偵測極限……………………………………………………… 41
(一)儀器偵測極限………………………………………………… 41
(二)方法偵測極限………………………………………………… 41
五、校正曲線法與標準添加法斜率之比較……………………… 41
六、參考樣品之驗證……………………………………………… 41
七、市售海藻類食品含量之分析………………………………… 42
(一)水分含量之分析……………………………………………… 42
(二)砷含量之分析………………………………………………… 42
伍、結論…………………………………………………………… 44
陸、參考文獻……………………………………………………… 45
柒、圖表…………………………………………………………… 54

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